تفاعل #1018586
ord-a7048d3bbfa14efa84ad26e2922eac4e
معادلة التفاعل
المتفاعلات
الكواشف
ظروف التفاعل
المعالجة
- 1أخرىA round-bottom flask equipped with a stirring bar, a reflux condenser and a dropping funnel
- 2درجة الحرارةthe reaction mixture was further heated to 90° C
- 3أخرىAfter completion of reaction
- 4درجة الحرارةthe reaction mixture was cooled down to 70-75° C.
- 5درجة الحرارةthe reaction mixture was further heated to 90-95° C
- 6أخرىAfter completion of reaction
- 7درجة الحرارةthe reaction mixture was cooled down again to 75° C.
- 8غسيلwashed with hot brine solution
- 9أخرىto remove traces of triethylamine
- 10ترشيحThe organic layer was filtered over Celite column
- 11أخرىto remove charcoal
- 12أخرىto remove traces of acrylic acid
- 13ترشيحThe organic phase was further filtered
- 14تركيزconcentrated
- 15أخرىto yield pale yellow color viscous product
الإجراء التجريبي
A round-bottom flask equipped with a stirring bar, a reflux condenser and a dropping funnel was charged with 1.6 g of 4-vinyl-1-cyclohexene 1,2-epoxide, and was heated to 70-75° C. At this point catalytic amount of platinum(0)-1,3-divinyl-1,1,3,3-tetramethyldisiloxane complex solution in xylene, (Pt around 2%) was added and the reaction mixture was further heated to 90° C. To this reaction mixture, 10 g of monohydride functionalized polydimethylsiloxane, was added drop-wise. After completion of reaction, the reaction mixture was cooled down to 70-75° C. and 20 mL of Toluene, and a catalytic amount of Titanium isopropoxide and TEMPO (2,2,6,6-Tetramethylpiperidine 1-oxyl) was added and the reaction mixture was further heated to 90-95° C. To this reaction mixture, 1.7 g of acrylic acid, was added drop-wise over a period of two hours. The reaction was monitored using 1H-NMR spectroscopy. After completion of reaction, the reaction mixture was cooled down again to 75° C. and 2.5 g of succinic anhydride, 2.5 g of triethylamine, and 300 ppm of hydroquinone was added. The reaction was monitored using 1H-NMR spectroscopy. After completion the product was vacuum striped, re-dissolved in dichloromethane and washed with hot brine solution. The organic phase was passed over Tulsion T66-MP resin to remove traces of triethylamine and decolorized using activated charcoal. The organic layer was filtered over Celite column to remove charcoal and then stirred along with Dowex WBA resin to remove traces of acrylic acid. The organic phase was further filtered and concentrated to yield pale yellow color viscous product.